HRID2223875

反应详情

EQUATION

反应方程式

HRID 2223875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-(1-benzylpiperidin-4-ylamino)-5-methylpyridine (11.3 g) in ethanol (250 mL) was added 20% palladium hydroxide (4 g). After stirring the solution at room temperature under hydrogen atmosphere for 48 hours, 20% palladium hydroxide (2 g) was further added. The solution was then stirred at room temperature under hydrogen atmosphere for additional 99 hours. The catalyst was filtered off. After concentration under reduced pressure, the resulting residue was purified by chromatography [NH silica gel, chloroform:methanol=10:1]. The resulting crude product was crystallized from ethyl acetate/hexane to give the title compound (5.97 g).

WORKUP

后处理

  1. stirringThe solution was then stirred at room temperature under hydrogen atmosphere for additional 99 hours
  2. filtrationThe catalyst was filtered off
  3. concentrationAfter concentration under reduced pressure
  4. customthe resulting residue was purified by chromatography [NH silica gel, chloroform:methanol=10:1]
  5. customThe resulting crude product was crystallized from ethyl acetate/hexane